CN111118607B - Hetero-anion nonlinear optical material and preparation method and application thereof - Google Patents
Hetero-anion nonlinear optical material and preparation method and application thereof Download PDFInfo
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- CN111118607B CN111118607B CN202010018498.XA CN202010018498A CN111118607B CN 111118607 B CN111118607 B CN 111118607B CN 202010018498 A CN202010018498 A CN 202010018498A CN 111118607 B CN111118607 B CN 111118607B
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Abstract
The invention relates to a kind of mixed anion nonlinear optical material and its preparation method and application, the chemical formula of the said mixed anion nonlinear optical material is Sr4Pb1.5Sb5O5Se8Is at the position ofCmMonoclinic compounds of space group.
Description
Technical Field
The invention relates to a hetero-anion nonlinear optical material and a preparation method and application thereof, belonging to the field of material preparation.
Background
The nonlinear optical crystal material refers to a crystal material having a frequency conversion effect, an electro-optic effect, a photorefractive effect and the like. When light propagates through the crystal, the optical electric field interacts with the crystal to cause electrical polarization of the crystal, thereby generating a polarization field, which in turn generates radiation light. When the light intensity is not large, the polarization field intensity and the photoelectric field intensity are in a linear relation, and when the laser light intensity is small, the second-order nonlinear term of the polarization coefficient cannot be ignored. Under the action of the secondary nonlinear coefficient, the radiation light generated by the nonlinear polarization field is not the frequency of the original incident light any more, and the wavelength is changed, so that the laser frequency conversion under the nonlinear optical effect can be realized. Nonlinear optical crystal materials are an important component of material science. The research on the nonlinear optical crystal material with reliable performance realizes laser conversion by utilizing the birefringence phase matching technology, and has important significance in converting light of mature technologies of other wave bands into laser output of special wave bands. In addition to frequency conversion, nonlinear optical materials also have important applications in the laser fields of signal transmission, optical information storage, photoelectric reactance and the like. The research on nonlinear optical materials has become a research hotspot in the fields of current international functional materials and the like.
In 1960, the first ruby (Cr) in the world was successfully studied by t.m. maiman3+:Al2O3) A pulsed laser; in 1961, p.a.franken laser-incident ruby on crystal (α -SiO)2) The frequency doubling effect generated by the crystal is discovered for the first time. From this point on, a new era of nonlinear optics and its material development was opened up.
At present, many problems exist in theory and application, but the potential huge commercial application prospect and micro mechanism of the method arouse wide interest, and the theory and application of the method have great research value.
Therefore, the invention aims to provide a hetero-anion nonlinear optical material with nonlinear optical effect, and a preparation method and application thereof.
Disclosure of Invention
In one aspect, the present invention provides a heteroanionic nonlinear optical material having a chemical formula of Sr4Pb1.5Sb5O5Se8A monoclinic compound located in the Cm space group.
The nonlinear optical crystal is the most critical component for adjusting the laser frequency. The chemical formula of the hetero anion nonlinear optical material prepared by the invention is Sr4Pb1.5Sb5O5Se8It is monoclinic system, belonging to non-centrosymmetric structure, and can make it possess non-linear optical effect. And the compound is black in color. The crystal structure of the compound can be clearly divided into two structural functional regions. The structure is composed of a plurality of∞ 2[Pb2Sb4Se9]2-A stack of layers, some anions Sr2+、∞ 1[SbO3]3-And SbO2 -Dispersed between the layers to separate adjacent layers.∞ 2[Pb2Sb4Se9]2-The layers are composed of distorted octahedra of Pb, Sb and Se respectively arranged co-edge with each other, and the ordered arrangement of these distorted octahedra can lead to polarity in the structure, which is responsible for the observed Second Harmonic (SHG) response.
In another aspect, the present invention further provides a method for preparing the above-mentioned hetero-anionic nonlinear optical material, comprising:
weighing raw materials SrSe, Pb and Sb according to the stoichiometric ratio of the heteroanionic nonlinear optical material2O3And Sb2Se3Mixing to obtain raw material powder;
and adding a fluxing agent into the obtained raw material powder, carrying out solid-phase reaction at 600-850 ℃ in a vacuum condition, and then cleaning and drying to obtain the hybrid anion nonlinear optical material.
Preferably, the fluxing agent is selected from at least one of CsI, KI, CsCl and KCl; the mass of the fluxing agent is 10-50 times of the total mass of the raw material powder.
Preferably, after adding a fluxing agent into the obtained raw material powder, the raw material powder is loaded into a quartz tube with the inner surface plated with carbon, and the upper end of the quartz tube is fused and packaged by oxyhydrogen flame under the vacuum condition.
Preferably, the vacuum condition is less than or equal to 10-2mbar。
Preferably, the temperature of the solid phase reaction is 750 ℃.
Preferably, the time of the solid phase reaction is 1000 to 4000 minutes, and is preferably 1400 minutes.
Preferably, after the solid phase reaction is finished, cooling to room temperature at a cooling rate of 1-10 ℃/hour; preferably, the cooling rate is 3 ℃/hour.
In still another aspect, the present invention also provides an application of the above-mentioned hetero-anion nonlinear optical material in the preparation of a laser frequency conversion device, an electro-optical switching device, or an optical information storage device.
Has the advantages that:
the hetero anion nonlinear optical material has a nonlinear optical effect, and the preparation method is simple to operate and easy for large-scale preparation. The prepared mixed anion nonlinear optical material is a new compound which is never reported, has a secondary frequency doubling effect, and is a potential material for preparing devices such as laser frequency conversion, electro-optical switches, optical information storage and the like.
Drawings
FIG. 1 is a crystal structure diagram of a heteroanionic nonlinear optical material obtained in example 1 of the present invention;
FIG. 2 is a diagram of the second harmonic generation performance of the polyanionic nonlinear optical material obtained in example 1 of the present invention;
FIG. 3 is a spectrum of the polyanionic nonlinear optical material obtained in example 1 of the present invention;
FIG. 4 is an XRD pattern of the heteroanionic nonlinear optical material obtained in example 1 of the present invention;
FIG. 5 is an XRD pattern of the heteroanionic nonlinear optical material obtained in example 2 of the present invention;
FIG. 6 is an XRD pattern of the heteroanionic nonlinear optical material obtained in example 3 of the present invention.
Detailed Description
The present invention is further illustrated by the following examples, which are to be understood as merely illustrative and not restrictive.
In the present disclosure, the chemical formula of the heteroanionic nonlinear optical material is Sr4Pb1.5Sb5O5Se8A completely new monoclinic compound located in the Cm space group.
In one embodiment of the invention, the heteroanionic nonlinear optical material is prepared by a molten salt-assisted solid-phase reaction method.
The following is an exemplary description of the process for preparing the heteroanionic nonlinear optical material provided by the present invention.
According to Sr4Pb1.5Sb5O5Se8Stoichiometric ratio is measured properlyRaw materials SrSe, Pb and Sb2O3And Sb2Se3And mixing to obtain a raw material powder mixture. The mixing may be by grinding in a mortar.
And adding at least one of CsI, KI, CsCl, KCl and the like into the raw material powder to be used as molten salt (fluxing agent), and uniformly mixing to obtain mixed powder. The mixing may be performed by grinding in a mortar. Wherein the mass of the molten salt is 10-50 times of the total mass of the raw material powder. The addition of the molten salt contributes to Sr at high temperature4Pb1.5Sb5O5Se8The crystal growth makes the obtained crystal have better quality, more regular shape (rod shape) and larger size.
And carrying out solid-phase reaction on the mixed powder under a vacuum condition, and then cleaning and drying to obtain the mixed anion nonlinear optical material. Wherein the vacuum condition is 10-2mbar or less. Or the mixed powder is put into a quartz tube with the inner surface plated with carbon, and the upper end of the quartz tube is melted and packaged by oxyhydrogen flame under the vacuum condition, so that the vacuum condition in the quartz tube is less than 102 mbar. The temperature of the solid phase reaction may be 600 to 850 ℃, preferably 600 to 800 ℃, for example 750 ℃. The time of the solid phase reaction can be 1000-4000 min, such as 1440 min. So that the mixed powder can reach enough reaction temperature at high temperature and have enough time to react to form a phase, thereby avoiding that the mixed powder is too low in temperature and difficult to react or too short in time and impure in product.
In an alternative embodiment, the solvent used for the washing is at least one of deionized water, DMF, NMP, and ethanol. The drying temperature can be 25-80 ℃ and the drying time can be 2-8 hours.
In an optional embodiment, after the solid-phase reaction is finished, cooling is carried out at a cooling speed of 1-10 ℃/hour, so that the aim of slowly cooling is to obtain crystals with better quality and larger size.
As a detailed example of the preparation of the heteroanionic nonlinear optical crystal, the method comprises the following steps: the mixed powder is firstly put into a quartz tube with the inner surface plated with carbon, and the upper end of the quartz tube is burned and sealed by oxyhydrogen flame under the vacuum condition. Subsequently, the quartz tube is placed in a muffle furnace, and thenPerforming solid-phase reaction at 600-850 ℃, cooling to room temperature at 3 ℃/h, and taking out the quartz tube. Further breaking the quartz tube, washing the obtained sample by deionized water to remove the fluxing agent, and obtaining Sr4Pb1.5Sb5O5Se8And (3) single crystal.
In the present invention, a hetero-anionic nonlinear optical crystal (Sr)4Pb1.5Sb5O5Se8) Can be used for frequency conversion of laser output from infrared to ultraviolet region. More specifically, the material of the invention adopts a reflection mode test under 2.09 μm laser irradiation to obtain a sharp downward SHG peak with the signal intensity about that of the commercial nonlinear material AgGaS20.25 times of.
The present invention will be described in detail by way of examples. It is also to be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the invention, and that certain insubstantial modifications and adaptations of the invention by those skilled in the art may be made in light of the above teachings. The specific process parameters and the like of the following examples are also only one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below.
Example 1
Weighing 1mol of SrSe, 0.375mmol of Pb and 0.42mmol of Sb as raw materials according to the stoichiometric ratio2O3、0.21mmol Sb2Se3And 0.375mmol Se, then adding 1.5g CsI as molten salt, and uniformly grinding in a mortar to obtain mixed powder.
The obtained mixed powder was put into a quartz tube with an inner surface coated with carbon, and the degree of vacuum was 10-2And (5) burning, melting and packaging the upper end of the quartz tube by using oxyhydrogen flame under the condition of mbar.
The quartz tube is put into a muffle furnace, heated to 750 ℃, kept at the temperature for 1400min, cooled at the speed of 3 ℃/h and taken out. The quartz tube is broken and cleaned by deionized water to remove the fluxing agent, and then Sr is obtained4Pb1.5Sb5O5Se8The single crystal of (1).
Sample characterization
The method comprises the steps of collecting single crystal sample structure information by using an X-ray single crystal diffractometer, collecting powder sample structure information by using a powder X-ray diffractometer, testing sample related spectra by using an ultraviolet spectrometer, and testing secondary frequency doubling effect by using a laser powder frequency doubling instrument.
As a result of the crystal structure of the hetero-anionic nonlinear optical material obtained in example 1, as shown in FIG. 1, (a) is Sr4Pb1.5Sb5O5Se8The crystal structure of (a); (b) is [ PbSbO ] viewed from the c-axis direction4]3-Chain structure diagram. The structure is obtained by collecting data through a D8QUEST single crystal diffractometer produced by Bruker, Germany, and refining through APEX3 software carried by the diffractometer4Pb1.5Sb5O5Se8The crystal data and the refinement data of (a) are shown in table 1.
The second harmonic generation performance (SHG) test result of the heteroanionic nonlinear optical material obtained in this example 1, as shown in fig. 2, shows that the compound has very excellent nonlinear optical effect.
The spectrum test result of the hetero-anionic nonlinear optical material obtained in this example 1 is shown in FIG. 3, where FIG. 3 is F1/2The hv curve, the inset is the absorption percentage versus wavelength curve, and it can be seen from fig. 3 that after 1400nm, the sample absorbs a small amount of photons and the transmittance is high. The optical band gap of this compound was estimated to be 0.919eV by using the Kubelka-Munk equation.
Table 1 shows Sr obtained in example 14Pb1.5Sb5O5Se8Crystal data and refinement data of (c):
example 2
Weighing 1mol of SrSe, 0.375mmol of Pb and 0.42mmol of Sb as raw materials according to the stoichiometric ratio2O3、0.21mmol Sb2Se3And 0.375mmol Se, then adding 1.5g CsI as molten salt, and uniformly grinding in a mortar to obtain mixed powder.
The obtained mixed powder was put into a quartz tube with an inner surface coated with carbon, and the degree of vacuum was 10-2And (5) burning, melting and packaging the upper end of the quartz tube by using oxyhydrogen flame under the condition of mbar.
The quartz tube is put into a muffle furnace, heated to 850 ℃, kept at the temperature for 1400min, cooled at the speed of 3 ℃/h and taken out. The quartz tube is broken and cleaned by deionized water to remove the fluxing agent, and then Sr is obtained4Pb1.5Sb5O5Se8The single crystal of (1).
Sample characterization
And collecting the structural information of the powder sample by using a powder X-ray diffractometer.
The result of the powder XRD test of the obtained heteroanionic nonlinear optical material of example 2. Where line 1 is the XRD pattern obtained by computational simulation and line 2 is the XRD pattern obtained for the material obtained in example 2, the comparison shows that the sample is phase pure.
Example 3
Weighing 1mol of SrSe, 0.375mmol of Pb and 0.42mmol of Sb as raw materials according to the stoichiometric ratio2O3、0.21mmol Sb2Se3And 0.375mmol Se, then adding 1.0g CsI as molten salt, and uniformly grinding in a mortar to obtain mixed powder.
The obtained mixed powder was put into a quartz tube with an inner surface coated with carbon, and the degree of vacuum was 10-2And (5) burning, melting and packaging the upper end of the quartz tube by using oxyhydrogen flame under the condition of mbar.
The quartz tube is put into a muffle furnace, heated to 750 ℃, kept at the temperature for 1400min, cooled at the speed of 3 ℃/h and taken out. The quartz tube is broken and cleaned by deionized water to remove the fluxing agent, and then Sr is obtained4Pb1.5Sb5O5Se8The single crystal of (1).
Sample characterization
And collecting the structural information of the powder sample by using a powder X-ray diffractometer.
The result of the powder XRD test of the obtained heteroanionic nonlinear optical material of example 3. Where line 1 is the XRD pattern obtained by computational simulation and line 2 is the XRD pattern obtained for the material obtained in example 2, the comparison shows that the sample is phase pure.
Claims (11)
1. A heteroanionic nonlinear optical material, wherein the chemical formula of the heteroanionic nonlinear optical material is Sr4Pb1.5Sb5O5Se8Is at the position ofCmA monoclinic compound of the space group; the hetero-anionic nonlinear optical material consists of∞ 2[Pb2Sb4Se9]2-Layers are stacked, wherein the anion Sr2+、∞ 1[SbO3]3-And SbO2 -Dispersed between the layers to separate adjacent layers; the above-mentioned∞ 2[Pb2Sb4Se9]2-The layer is formed by arranging distorted octahedrons formed by Pb, Sb and Se in a mutual sharing way.
2. A method for preparing the heteroanionic nonlinear optical material of claim 1, which comprises:
weighing raw materials SrSe, Pb and Sb according to the stoichiometric ratio of the heteroanionic nonlinear optical material2O3And Sb2Se3Mixing to obtain raw material powder;
adding a fluxing agent into the obtained raw material powder, carrying out solid-phase reaction at 600-850 ℃ in a vacuum condition, and then cleaning and drying to obtain the hybrid anion nonlinear optical material; the fluxing agent is selected from at least one of CsI, KI, CsCl and KCl.
3. The preparation method according to claim 2, wherein the mass of the flux is 10 to 50 times of the total mass of the raw material powder.
4. The production method according to claim 2, wherein a flux is added to the raw material powder, and the raw material powder is loaded into a quartz tube having a carbon-plated inner surface, and the quartz tube is sealed by fusing the upper end thereof with an oxyhydrogen flame under vacuum.
5. The method according to claim 2, wherein the vacuum condition is 10 or less-2 mbar。
6. The method according to claim 2, wherein the temperature of the solid phase reaction is 750 ℃.
7. The method according to claim 2, wherein the time for the solid phase reaction is 1000 to 4000 minutes.
8. The method according to claim 7, wherein the time for the solid phase reaction is 1400 minutes.
9. The method according to any one of claims 2 to 8, wherein the temperature is decreased to room temperature at a rate of 1 to 10 ℃/hr after the completion of the solid phase reaction.
10. The method of claim 9, wherein the cooling rate is 3 ℃/hr.
11. Use of a heteroanionic nonlinear optical material described in claim 1 for the preparation of a laser frequency conversion device, an electro-optical switching device, or an optical information storage device.
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